CN116119742A - Low-resistance cobalt-coated ball nickel oxidation method - Google Patents
Low-resistance cobalt-coated ball nickel oxidation method Download PDFInfo
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- CN116119742A CN116119742A CN202310230425.0A CN202310230425A CN116119742A CN 116119742 A CN116119742 A CN 116119742A CN 202310230425 A CN202310230425 A CN 202310230425A CN 116119742 A CN116119742 A CN 116119742A
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- cobalt
- coated
- caustic soda
- low
- stirring
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 35
- 239000010941 cobalt Substances 0.000 title claims abstract description 35
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 114
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 229910018916 CoOOH Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001869 cobalt compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a low-resistance cobalt-coated ball nickel oxidation method, which comprises the following steps: (1) Adding caustic soda flakes into pure water to prepare caustic soda liquid with the concentration of 60-70%; (2) Adding cobalt-coated materials into a reactor with the addition amount of 200-300kg, and then adding 6-10L of liquid alkali obtained in the step (1); (3) The temperature of the reactor is raised to more than 80 ℃, oxygen is introduced, and the flow is 10-20m 3 And/h, stirring for at least 25min to finish the oxidation.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a low-resistance cobalt-coated ball nickel oxidation method.
Background
The low-resistance cobalt-coated positive electrode material is mainly used as a positive electrode material of a new energy battery, a layer of Co (OH) 2 is formed on the surface of spherical Ni (OH) 2 particles through coating reaction, the coating layer is oxidized into CoOOH through an oxidation process, polarization overpotential in the nickel positive electrode oxidation process is eliminated or inhibited, the difference between the oxidation potential and the oxygen evolution potential is increased, cobalt compounds are prevented from being dissolved, and the charge and substance exchange capacity in the electrochemical process is improved. However, the conventional oxidation method has high resistance of oxidized materials, the coating layer is not completely oxidized, and part of the matrix nickel hydroxide is oxidized, so that the electrochemical performance of the material is seriously affected. The invention aims to provide a novel cobalt-coated ball nickel oxidation method which has the advantages of simplicity and convenience in operation, low resistance of prepared materials and the like.
Disclosure of Invention
Aiming at the technical problems, the invention provides a low-resistance cobalt-coated ball nickel oxidation method.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the low-resistance cobalt-coated ball nickel oxidation method comprises the following steps:
(1) Adding caustic soda flakes into pure water to prepare caustic soda liquid with the concentration of 60-70%;
(2) Adding cobalt-coated materials into a reactor with the addition amount of 200-300kg, and then adding 6-10L of liquid alkali obtained in the step (1);
(3) The temperature of the reactor is raised to more than 80 ℃, oxygen is introduced, and the flow is 10-20m 3 And/h, stirring for at least 25min to finish the oxidation.
Wherein, in the step (1), the preparation process is that caustic soda flakes are added into pure water with the addition amount of 1.5-2.5kg/L, stirring is started, and stirring is continued for 0.5 hour for standby.
Wherein in the step (3), the temperature of the reactor is raised to 80-120 ℃.
Wherein in the step (3), the stirring time is 25-35min.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
The beneficial effects of the invention are as follows: the method adds the high-concentration liquid alkali in the oxidation process, ensures that Co 2+ Fully oxidize to Co 3+ An external circulation conductive network is formed, the introduction of water is reduced by high-concentration liquid alkali, excessive oxidation is prevented by oxygen flow distributed introduction, and Co with embedded internal structure is formed 2+ Is not oxidized, ensures an internal circulation conductive network, saves the addition amount of oxygen and saves the cost. The invention overcomes the defects of incomplete oxidation and high resistance of the existing cobalt-coated ball nickel, and provides a novel cobalt-coated ball nickel oxidation method which has the advantages of simple operation, thorough oxidation of a coating layer, low resistance of a prepared material, good conductivity and the like.
Detailed Description
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Example 1
The low-resistance cobalt-coated ball nickel oxidation method comprises the following steps:
(1) Adding caustic soda flakes into pure water to prepare caustic soda liquid with the concentration of 60%;
(2) Adding cobalt-coated materials into a reactor with the addition amount of 200kg, and then adding 6L of liquid alkali obtained in the step (1);
(3) The temperature of the reactor is raised to 80 ℃, oxygen is introduced, and the flow is 10m 3 And (3) stirring for 25min to finish oxidation, wherein the tabletting resistance of the oxidized material is lower than 3Ω under 6000 MPa.
In the step (1), the preparation process is that caustic soda flakes are added into pure water with the addition amount of 1.5kg/L, stirring is started, and stirring is continued for 0.5 hour for standby.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
Example 2
The low-resistance cobalt-coated ball nickel oxidation method comprises the following steps:
(1) Adding caustic soda flakes into pure water to prepare caustic soda liquid with the concentration of 70%;
(2) Adding cobalt-coated materials into a reactor with the addition amount of 300kg, and then adding 10L of liquid alkali obtained in the step (1);
(3) The temperature of the reactor is raised to 120 ℃, oxygen is introduced, and the flow is 20m 3 And (3) stirring for 35min to finish oxidization, wherein the tabletting resistance of the oxidized material is lower than 3Ω under 6000 MPa.
In the step (1), the preparation process is that caustic soda flakes are added into pure water with the addition amount of 2.5kg/L, stirring is started, and stirring is continued for 0.5 hour for standby.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
Example 3
A low-resistance cobalt-coated ball nickel oxidation method comprises the following specific steps:
(1) Adding caustic soda flakes into pure water with the addition amount of 2.0kg/L, starting stirring, and continuously stirring for 0.5 hours for standby to obtain liquid caustic soda with the concentration of 67%;
(2) Adding cobalt-coated materials into a reaction kettle, wherein the addition amount is 250kg, and adding 8L of the liquid alkali prepared in the step (1);
(3) Heating to 80 ℃, starting oxygen with the oxygen flow of 15m 3 And (3) stirring for 30min to finish oxidation, wherein the tabletting resistance of the oxidized material is lower than 3Ω under 6000MPa pressure.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
Example 4
A low-resistance cobalt-coated ball nickel oxidation method comprises the following specific steps:
(1) Adding caustic soda flakes into pure water with the addition amount of 2.3kg/L, starting stirring, and continuously stirring for 0.5 hour for standby to obtain caustic soda liquid with the concentration of 70%;
(2) Adding cobalt-coated materials into a reaction kettle, wherein the addition amount is 300kg, and adding 10L of the liquid alkali prepared in the step (1);
(3) Heating to 100deg.C, and opening oxygen with flow rate of 20m 3 And (3) stirring for 35min to finish oxidization, wherein the tabletting resistance of the oxidized material is lower than 3Ω under 6000 MPa.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
Example 5
A low-resistance cobalt-coated ball nickel oxidation method comprises the following specific steps:
(1) Adding caustic soda flakes into pure water with the addition amount of 2.0kg/L, starting stirring, and continuously stirring for 0.5 hours for standby to obtain liquid caustic soda with the concentration of 67%;
(2) Adding cobalt-coated materials into a reaction kettle, wherein the addition amount is 300kg, and adding 6L of the liquid alkali prepared in the step (1);
(3) Heating to 120deg.C, and opening oxygen with oxygen flow of 20m 3 Stirring for 10min to reduce oxygen flow to 10m 3 And (3) stirring for 20min again after the step/h, and finishing oxidation, wherein the tabletting resistance of the oxidized material is lower than 3 omega under the pressure of 6000 MPa.
In the step (1), the purity of the caustic soda flakes must reach 99%, so that the caustic soda flakes are prevented from influencing the purity of the prepared caustic soda flakes and the quality of finished products.
Wherein in the step (2), the moisture of the added cobalt-coated material is required to be less than 1%.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explanation of the principles of the present invention and are in no way limiting of the invention. Accordingly, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention. Furthermore, the appended claims are intended to cover all such changes and modifications that fall within the scope and boundary of the appended claims, or equivalents of such scope and boundary.
Claims (6)
1. The low-resistance cobalt-coated ball nickel oxidation method is characterized by comprising the following steps of:
(1) Adding caustic soda flakes into pure water to prepare caustic soda liquid with the concentration of 60-70%;
(2) Adding cobalt-coated materials into a reactor with the addition amount of 200-300kg, and then adding 6-10L of liquid alkali obtained in the step (1);
(3) The temperature of the reactor is raised to more than 80 ℃, oxygen is introduced, and the flow is 10-20m 3 And/h, stirring for at least 25min to finish the oxidation.
2. The method for oxidizing nickel coated with cobalt balls with low resistance according to claim 1, wherein in the step (1), the configuration process is that caustic soda flakes are added into pure water with the addition amount of 1.5-2.5kg/L, stirring is started, and stirring is continued for 0.5 hour for later use.
3. The method for oxidizing low-resistance cobalt-coated sphere nickel according to claim 1, wherein in the step (3), the temperature of the reactor is raised to 80-120 ℃.
4. The method for oxidizing nickel coated with cobalt balls with low resistance according to claim 1 or 3, wherein in the step (3), the stirring time is 25-35min.
5. The method for oxidizing low-resistance cobalt-coated sphere nickel according to claim 1, wherein in the step (1), the purity of the flake alkali must reach 99%, so that the purity of the flake alkali is prevented from being insufficient to influence the purity of the prepared liquid alkali and influence the quality of a finished product.
6. The method of claim 1, wherein in step (2), the moisture of the added cobalt-coated material is less than 1%.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101106193A (en) * | 2007-07-09 | 2008-01-16 | 金天能源材料有限公司 | Preparation method of nickel hydroxide with surface coated with gamma-hydroxy cobalt oxide |
CN102142547A (en) * | 2011-01-29 | 2011-08-03 | 江门市长优实业有限公司 | Preparation method of spherical nickel hydroxide anode material coated with gamma-hydroxy cobalt oxide |
CN102509788A (en) * | 2011-11-04 | 2012-06-20 | 安徽亚兰德新能源材料股份有限公司 | Dry gaseous oxidation preparation of spherical cobalt-coated nickel hydroxide |
CN102800859A (en) * | 2012-08-30 | 2012-11-28 | 上海锦众信息科技有限公司 | Preparation method of cobalt-wrapped nickelous hydroxide |
CN103199241A (en) * | 2013-04-26 | 2013-07-10 | 先进储能材料国家工程研究中心有限责任公司 | Method for preparing spherical nickel hydroxide with surface being coated with gamma CoOOH |
CN110828791A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Anti-oxidation method in coating reaction process of cobalt-coated positive electrode material |
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2023
- 2023-03-11 CN CN202310230425.0A patent/CN116119742A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101106193A (en) * | 2007-07-09 | 2008-01-16 | 金天能源材料有限公司 | Preparation method of nickel hydroxide with surface coated with gamma-hydroxy cobalt oxide |
CN102142547A (en) * | 2011-01-29 | 2011-08-03 | 江门市长优实业有限公司 | Preparation method of spherical nickel hydroxide anode material coated with gamma-hydroxy cobalt oxide |
CN102509788A (en) * | 2011-11-04 | 2012-06-20 | 安徽亚兰德新能源材料股份有限公司 | Dry gaseous oxidation preparation of spherical cobalt-coated nickel hydroxide |
CN102800859A (en) * | 2012-08-30 | 2012-11-28 | 上海锦众信息科技有限公司 | Preparation method of cobalt-wrapped nickelous hydroxide |
CN103199241A (en) * | 2013-04-26 | 2013-07-10 | 先进储能材料国家工程研究中心有限责任公司 | Method for preparing spherical nickel hydroxide with surface being coated with gamma CoOOH |
CN110828791A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Anti-oxidation method in coating reaction process of cobalt-coated positive electrode material |
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Effective date of registration: 20240411 Address after: 737104 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province Applicant after: Jinchuan Group Nickel Cobalt Co.,Ltd. Country or region after: China Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Applicant before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |
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